基于氧化铁模板原位制备Ni/Fe-LDHs/Fe薄膜及其性能研究
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摘要
采用模版原位生长技术,以NH_3·H_2O调节Ni(NO_3)_2-NH_4NO_3反应溶液pH值,形成镍氨配离子达到缓慢释放Ni~(2+),实现了在阳极氧化铁模板(AFO/Fe)上制备Ni/Fe-NO_3-LDHs/Fe薄膜前驱体;然后,通过离子交换反应将磺基水杨酸阴离子(SSA)插层制备了Ni/Fe-SSA-LDHs/Fe复合薄膜。借助XRD、FT-IR、SEM、UV-Vis、TG/DTA及电化学测试等手段对LDHs薄膜结构及性能进行了表征与分析。结果显示,SSA阴离子插入LDHs层间,插层距由0.9051 nm扩至1.1837 nm,水滑石晶片主要以c轴平行于氧化铁模版生长。该薄膜表现出优异的耐蚀性和紫外阻隔性能。
A Ni/Fe-NO_3-LDHs/Fe film was prepared on anodized Fe substrate by template in-situ growth method. The pH of the reaction solution was adjusted by NH_3·H_2O to release Ni~(2+) slowly by the formation of nickel-ammonia complexion. Sulfosalicylic acid anion intercalated Ni/Fe-SSA-LDHs/Fe composite film was synthesized through ion-exchange method using the Ni/Fe-NO_3-LDHs/Fe film as precursor. The prepared film was investigated by XRD, FT-IR, SEM,UV-Vis,TG/DTA and electrochemical test. The results confirmed the successful incorporation of SSA anions into the interlayer galleries of NI/Fe-LDHs with an expansion of d-spacing from 0.9051 to 1.1837 nm. The LDHs films were mainly oriented with the c axis of the platelet crystallites parallel to the substrate surface. The results indicated that the as-prepared LDHs films possessed excellent corrosion-resistant and UV absorption properties.
A Ni/Fe-NO_3-LDHs/Fe film was prepared on anodized Fe substrate by template in-situ growth method. The pH of the reaction solution was adjusted by NH_3·H_2O to release Ni~(2+) slowly by the formation of nickel-ammonia complexion. Sulfosalicylic acid anion intercalated Ni/Fe-SSA-LDHs/Fe composite film was synthesized through ion-exchange method using the Ni/Fe-NO_3-LDHs/Fe film as precursor. The prepared film was investigated by XRD, FT-IR, SEM,UV-Vis,TG/DTA and electrochemical test. The results confirmed the successful incorporation of SSA anions into the interlayer galleries of NI/Fe-LDHs with an expansion of d-spacing from 0.9051 to 1.1837 nm. The LDHs films were mainly oriented with the c axis of the platelet crystallites parallel to the substrate surface. The results indicated that the as-prepared LDHs films possessed excellent corrosion-resistant and UV absorption properties.
引文
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[19] Zhang Weifeng,Li Dianqing,Sun Meng,et al.Supramolecular assembly of methyl orange-pillared hydrotalcite and its light and thermal stability[J].Chemical Journal of Chinese Universities,2004,25(10):1799-1803(in Chinese).张伟锋,李殿卿,孙勐,等.超分子结构甲基橙插层水滑石的组装及其光热稳定性研究[J].高等学校化学学报,2004,25(10):1799-1803.
[2] Qiu Mande,Niu Miao,Wang Yidan,et al.Study on the synthesis,microstructure and adsorption performance of nano-meter Mg-Al hydrotalcite[J].Journal of Synthetic Crystals,2016,45(4):1047-1054(in Chinese).仇满德,牛苗,王亦丹,等.纳米镁铝水滑石的合成、微结构及吸附性能研究[J].人工晶体学报,2016,45(4):1047-1054.
[3] Wang Z,Jia W,Jiang M L,et al.Microwave-assisted synthesis of layer-by-layer ultra-large and thin NiAl-LDH/RGO nanocomposites and their excellent performance as electrodes[J].Science China Materials,2015,58:944-952.
[4] Pan Dengke,Zhang Hui.Synthesis and characterization of magnetic Mg-Al mixed oxides submicro particles with core-shell structure[J].Chinese Journal of Inorganic Chemistry,2011,27(7):1341-1347(in Chinese).盘登科,张慧.核壳结构磁性镁铝复合氧化物亚微米粒子的制备与表征[J].无机化学学报,2011,27(7):1341-1347.
[5] Román M S S,Holgado M J,Salinas B,et al.Drug release from layered double hydroxides and from their polylactic acid (PLA) nanocomposites[J].Applied Clay Science,2013,71:1-7.
[6] Chen Hongyun,Xu Sailong,Chen Xu,et al.Research progress of layered double hydroxyl composite metal oxide thin films [J].Science in China (Series B:Chemistry),2008,38(8):659-667(in Chinese).陈虹芸,徐赛龙,陈旭,等.层状双羟基复合金属氢氧化物薄膜的研究进展[J].中国科学B辑:化学,2008,38(8):659-667.
[7] Chen Qiuhua.Studies on the reaction of L-cysteine in a confined matrix of layered double hydroxides and primary studies on the catalysis properties of layered double hydroxides films[D].Beijing:Beijing University of Chemical Technology,2009(in Chinese).陈秋华.半胱氨酸插层水滑石的层间反应研究及类水滑石薄膜的催化性能研究[D].北京:北京化工大学,2009.
[8] Wang Y L,Zhang D D.Electrocatalytic oxidation of methanol at Ni-Al layered double hydroxide film modi?ed electrode in alkaline medium[J].Electrochimica Acta,2011,56:5754-5758.
[9] Yin Z J,Wu J J.Amperometric sensors based on Ni/Al and Co/Al layered double hydroxide modified electrode and their application for hydrogen peroxide detection[J].Biosensors and Bioelectronics,2011,26:1970-1974.
[10] Peng Z C.Research progress of LDHs nanomaterials in anti-corrosion film[J].Total Corrosion Control,2014,28(6):18-21.
[11] Lu S X,Chen Y L.Controlled growth of superhydrophobic films by sol-gel method on aluminum substrate[J].Applied Surface Science,2010,256:6072-6075.
[12] Chen H,Zhao X,Gao H,et al.Synthesis of red light-emitting hydrotalcite-like compound and its application in LED[J].Chemical Journal of Chinese Universities,2015,36(6):41-47.
[13] Zhang B.Assembly of electrochemical luminescence molecules/layered double hydroxide ultrathin films and their application in sensors[D].Beijing:Beijing University of Chemical Technology,2012.
[14] Zhang Yingchao.Study on the fabrication and magnetic properties of oriented spinel type films derived from layered double hydroxide precursors[D].Beijing:Beijing University of Chemical Technology,2010 (in Chinese).张英超.取向尖晶石基薄膜的层状前驱体法制备及其磁学性能研究[D].北京:北京化工大学,2010.
[15] Wang Tianlei,Liu Meitang,Ma Hongwen.Recent advances in thin-film material based on layered double hydroxides via a layer-by-layer self-assembly method[J].Chemical Industry and Engineering Progress,2013,32(7):1584-1603.
[16] Guo X X,Zhang F Z,David G,et al.Layered double hydroxide films:synthesis,properties and applications[J].Chem Commun,2010,46:5197-5210.
[17] Zhao Ce,Zeng Hongyan,Wang Yaju,et al.“Memory effect” of Mg-Al hydrotalcites and its chromium(VI) adsorptionproperty[J].Journal of Inorganic Materials,2011,26(8):874-880(in Chinese).赵策,曾虹燕,王亚举,等.Mg-Al 水滑石“记忆效应”及其对Cr(VI)阴离子吸附性能研究[J].无机材料学报,2011,26(8):874-880.
[18] Li Dianqing,Feng Tao,Evans D G,et al.Assembly and structural characteristics of organic anion-pillared hydrotalcites[J].The Chinese Journal of Process Engineering,2002,2(4):355-360(in Chinese).李殿卿,冯桃,Evans D G,等.有机阴离子柱撑水滑石的插层组装及超分子结构[J].过程工程学报,2002,2(4):355-360.
[19] Zhang Weifeng,Li Dianqing,Sun Meng,et al.Supramolecular assembly of methyl orange-pillared hydrotalcite and its light and thermal stability[J].Chemical Journal of Chinese Universities,2004,25(10):1799-1803(in Chinese).张伟锋,李殿卿,孙勐,等.超分子结构甲基橙插层水滑石的组装及其光热稳定性研究[J].高等学校化学学报,2004,25(10):1799-1803.
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